CN108435223A - A kind of Catalyst For Propane Ammoxidation of P Modification and its preparation method and application - Google Patents

A kind of Catalyst For Propane Ammoxidation of P Modification and its preparation method and application Download PDF

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CN108435223A
CN108435223A CN201810386207.5A CN201810386207A CN108435223A CN 108435223 A CN108435223 A CN 108435223A CN 201810386207 A CN201810386207 A CN 201810386207A CN 108435223 A CN108435223 A CN 108435223A
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catalyst
modification
propane ammoxidation
preparation
salt
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CN108435223B (en
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林敬东
林锦汉
郭杰
万焱
许明亮
王勇
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Xiamen University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/14—Phosphorus; Compounds thereof
    • B01J27/186—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J27/195—Phosphorus; Compounds thereof with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium with vanadium, niobium or tantalum
    • B01J27/198—Vanadium
    • B01J27/199—Vanadium with chromium, molybdenum, tungsten or polonium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/002—Mixed oxides other than spinels, e.g. perovskite
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08—Heat treatment
    • B01J37/10—Heat treatment in the presence of water, e.g. steam
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/12—Oxidising
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C253/00—Preparation of carboxylic acid nitriles
    • C07C253/24—Preparation of carboxylic acid nitriles by ammoxidation of hydrocarbons or substituted hydrocarbons
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts

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  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
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  • Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a kind of Catalyst For Propane Ammoxidation of P Modification and its preparation method and application, the chemical general formula of the catalyst is Pa‑MobVcTedNbeOx, wherein 0.0001≤a≤1,0.1≤b≤1,0.1≤c≤1,0.1≤d≤1,0.1≤e≤1.The catalyst can be by by Mo salting liquids, Te salting liquids, and V salting liquids and Nb salting liquids carry out hydro-thermal reaction after being uniformly mixed and catalyst precursor are made；Then by the catalyst precursor by using infusion process to can be prepared by the catalyst with phosphorus doping after dioxygen water process.The present invention prepares the catalytic activity that high-performance MoVTeNb catalyst then further promotes catalyst by P Modification using hydro-thermal method and dioxygen water process.The preparation method of catalyst provided by the present invention has the advantages that simple and reproducible.In addition, catalyst provided by the present invention also has many advantages, such as higher conversion ratio and acrylonitrile selectivity for propane ammoxidation reaction.

Description

A kind of Catalyst For Propane Ammoxidation of P Modification and its preparation method and application
Technical field
The invention belongs to catalyst preparation and applied technical fields, and in particular to a kind of propane ammoxidation catalysis of P Modification Agent and its preparation method and application.
Background technology
Acrylonitrile is a kind of important industrial chemicals, it is three big synthetic materials --- synthetic fibers, synthetic rubber, plastics Important source material, it is widely used in organic synthesis industry and people's economic life.Currently, the whole world be more than 90% acrylonitrile all It is Sohio methods, i.e., propylene ammmoxidation process is come what is produced, and yield is up to 80%；However, since the price of propylene is the 3 of propane ~6 times, and influenced with upstream industry chain due to being restricted by petroleum resources, cost of investment day of the propylene as the raw material of ammoxidation Benefit improves.Propane is derived from a wealth of sources due to cheap, therefore is a kind of very potential and economic value acrylonitrile synthesis road Line.
People pass through long-term exploration, mainly have MoV serial at present, VSb series and VPO catalyst series can be applied to third Alkane ammoxidation reaction prepares acrylonitrile；Wherein, the MoVTeNb catalyst in MoV series is before most being applied in current report A kind of catalyst of scape, maximum output is up to 62% (US Patent 5,472,925 (1995), US Patent 6,063,728 (2000), Topics in Catalysis 23 (2003) pp 5-22.), M1 phases and M2 phases are contained in the catalyst (activity of MoVTeNbO catalyst is mutually made of the MoVTeNbO (M2) of the MoVTeNbO (M1) of orthogonal type and false six squares).Its Middle M1 has propane oxide dehydrogenation to propylene, is then catalyzed ammoxidation of propylene to the ability of acrylonitrile, and M2 phases are due to lacking V5+, Propane can not be activated, however it has efficient catalysis ammoxidation of propylene to the reactivity of acrylonitrile), optimal proportion is M1:M2=60:40(Topics in Catalysis 23(2003)pp 5-22).However it is different due to preparation condition, it urges The formation of agent active sites can be by various reaction conditions such as, solution pH value, metal salt presoma, the conditions such as drying mode and roasting Extreme influence, catalyst it is less reproducible.Therefore develop a kind of high-performance and the preparation method of catalyst that easily repeats still It is so a great difficult problem.
Invention content
Place in view of the deficiency of the prior art, present invention aims at provide a kind of propane ammonia oxygen of P Modification Change catalyst and its preparation method and application.
In order to achieve the above objectives, solution of the invention is：
A kind of Catalyst For Propane Ammoxidation of P Modification, it is characterised in that its chemical general formula is Pa-MobVcTedNbeOx, In 0.0001≤a≤1,0.1≤b≤1,0.1≤c≤1,0.1≤d≤1,0.1≤e≤1.
A kind of preparation method of the Catalyst For Propane Ammoxidation of P Modification as described in claim 1, it is characterised in that tool Steps are as follows for body：
1) Mo salt and Te salt are dissolved in the water and solution A is made；
2) V salt is dissolved in the water and solution B is made；
3) Nb salt is dissolved in the water and solution C is made；
4) solution B is added in solution A to and is stirred to obtain mixed solution, institute can be prepared by adding solution C stirring State the slurry of catalyst；
5) slurry of catalyst obtained in step 4) is subjected to hydro-thermal reaction；Reaction product is through being filtered, washed and drying Catalyst precursor is made；
6) catalyst precursor obtained in step 5) is subjected to calcination process；
7) by the catalyst precursor H after roasting in step 6)2O2It is handled；
8) by H in step 7)2O2Treated, and catalyst precursor can be prepared by the phosphorus by infusion process with phosphorus doping changes The Catalyst For Propane Ammoxidation of property.
Preferably, the Mo salt described in step 1) is ammonium molybdate；The Te salt in telluric chloride and telluric acid one Kind.
Preferably, the V salt described in step 2) is selected from one kind of vanadic sulfate and ammonium metavanadate.
Preferably, the one kind of Nb salt in ammonium niobium oxalate, niobium oxalate and columbium pentachloride described in step 3).
Preferably, the hydrothermal reaction condition described in step 5) is：Reaction kettle is passed through nitrogen and purges 5~20 minutes in advance, Hydrothermal temperature is 175 DEG C, and the reaction time is 1~48 hour.
Preferably, the calcination process condition described in step 6) is：Carry out under an inert atmosphere, calcination temperature be 500~ 600 DEG C, roasting time is 1~10h.
Preferably, the H described in step 7)2O2Mass fraction be 1~10%.
A kind of application of the Catalyst For Propane Ammoxidation of P Modification in preparing acrylonitrile form propane ammoxidation.
The design principle of the present invention is as follows：
MoVTeNb catalyst containing M1+M2 phases when conversion ratio is low (<50%) there is the selection of higher acrylonitrile Property, however its propane conversion capability is relatively low.When conversion ratio is further promoted, it is easy to cause deep oxidation.Pass through dioxygen water process Obtained pure M1 phases MoVTeNb catalyst has higher propane activity of conversion, however after its conversion ratio is more than 80%, depth Oxidation is serious, COxSelectivity generally higher than 40%,
It is not high so as to cause acrylonitrile selectivity.MoVTeNb catalyst is carried out surface to be modified being most simply to have at present The method and its favorable repeatability of the improvement catalyst activity of effect.Phosphorus has more report for oxidative dehydrogenation (Science,322(2008),pp.77-78；Catalysis Today,142(2009),pp 215–219；
ChemCatChem, 5 (2013), pp 757-765), the modification of phosphorus can inhibit oxidative dehydrogenation anti-to a certain extent Answer middle generation deep oxidation.The present invention is modified the surface of pure M1 phase catalysts by phosphorus, is improving conversion ratio and selectivity Meanwhile the M1+M2 phase catalysts avoided prepare more difficult repetition, and the problems such as harsh is required to preparation condition.
Advantages of the present invention：
(1) hydro-thermal method and dioxygen water process is used to prepare high-performance MoVTeNb catalyst then by P Modification into one Step promotes the catalytic activity of catalyst.
(2) preparation method of catalyst provided by the present invention is simple and reproducible.
(3) catalyst provided by the present invention has higher conversion ratio and acrylonitrile selectivity for propane ammoxidation.
Specific implementation mode
Further below in conjunction with the embodiments with the present invention will be described in detail.It will similarly be understood that following embodiment is served only for this Invention is further described, and should not be understood as limiting the scope of the invention, specific quality, reaction time in example Also only it is an example in OK range with temperature, technological parameter etc., those skilled in the art is according to the present invention above-mentioned Some nonessential modifications and adaptations that content is made all belong to the scope of protection of the present invention.Particular technique is not specified in embodiment Or condition person, it is to be carried out according to technology or condition described in document in the art or according to product description.It is used Production firm person is not specified in reagent or instrument, is the conventional products that can be bought by market.
Embodiment
In all of the embodiments illustrated, the computational methods of conversion ratio and selectivity are as follows：
The propane molal quantity of conversion of propane (%)=reaction/propane feed molal quantity * 100%
The propane molal quantity * 100% of acrylonitrile molal quantity/reaction of acrylonitrile selectivity (%)=generation
The acrylonitrile molal quantity of acrylonitrile yield (%)=generation/propane feed molal quantity * 100%
Embodiment 1
The preparation of catalyst：
1) according to Mo：V：Te：Nb=1.00:0.30:0.17:0.12 molar ratio weighs 17.04g tetra- and is hydrated seven molybdenums respectively Sour ammonium, 7.33g vanadic sulfates, 3.77g telluric acids and 4.51g ammonium niobium oxalates.Weighed ammonium heptamolybdate and telluric acid are added to In 60mL deionized waters, being stirred 5~15 minutes at 80 DEG C makes it fully dissolve, and obtains solution A.By weighed vanadic sulfate It is added in 30mL deionized waters, being stirred 5~15 minutes at 80 DEG C makes it fully dissolve, and obtains solution B.By weighed grass Sour niobium ammonium is added in 30mL deionized waters, and being stirred 5~15 minutes at 80 DEG C makes it fully dissolve, and obtains solution C.
2) solution B is added in solution A, is stirred 8 minutes.
3) solution C is added in the mixed solution in step 2), continues stirring 10 minutes.
4) slurries that step 3) obtains are transferred in 200mL water heating kettle polytetrafluoroethylliner liners, are then bubbled 5 with nitrogen ~20 minutes, the oxygen of the inside is discharged, is then placed in baking oven, 175 DEG C of hydro-thermal reactions 48 hours.
5) slurries that step 4) obtains are filtered, deionized water washing, the then drying overnight at 80 DEG C.
6) solid for obtaining step 5), the lower 600 DEG C of calcination process of nitrogen 2 hours.
7) 7) catalyst obtained step 6) corresponds to 30mL 5%H according to every gram of catalyst2O2Dosimeter, weigh institute The catalyst A needed in the hydrogen peroxide for devoting respective volume, is stirred 5 hours at 60 DEG C.
8) solution in step 7) is filtered, deionization washing in 80 DEG C of drying overnight, obtains catalyst B.
9) it weighs 0.001g phosphoric acid (80wt%) to be dissolved in 3.0g deionized waters, be sufficiently stirred, it is made to be uniformly mixed.
10) it measures the phosphoric acid solution prepared in 0.3g steps 9) to be added drop-wise in the catalyst B obtained in 1g steps 8), fully Stirring, makes it be evenly distributed on catalyst B, then in 80 DEG C of drying.
11) powder for obtaining step 10) under a nitrogen 550 DEG C of processing 2 hours to get to this example catalyst
Embodiment 2
Vanadic sulfate in step 1) in embodiment 1 is replaced with into ammonium metavanadate, ammonium niobium oxalate replaces with niobium oxalate, then according to According to Mo：V：Te：Nb=1.0:0.3:0.17:0.12 molar ratio feeds intake；Calcination temperature in step 6) is 600 DEG C, place It is 10 hours to manage the time, and other conditions are constant to can be prepared by this example catalyst.
Embodiment 3
Ammonium niobium oxalate in step 1) in embodiment 1 is replaced with into columbium pentachloride, then according to Mo：V：Te：Nb=1.0: 1.0:0.1:1.0 molar ratio feeds intake；The calcination process time in step 6) becomes 5 hours, use quality in step 7) The H that score is 10%2O2, other conditions are constant to can be prepared by this example catalyst.
Embodiment 4
Telluric acid in step 1) in embodiment 1 is replaced with into telluric chloride then according to Mo：V：Te：Nb=0.1:0.1: 1.0:1.0 molar ratio feeds intake；Calcination temperature in step 6) becomes 500 DEG C, and processing time is 10 hours, in step 7) The H that use quality score is 1%2O2, other conditions are constant to can be prepared by this example catalyst.
Embodiment 5
Telluric acid in step 1) in embodiment 1 is replaced with into telluric chloride, ammonium niobium oxalate replaces with columbium pentachloride, then according to According to Mo：V：Te：Nb=1.0:0.1:1.0:0.1 molar ratio feeds intake；Calcination temperature in step 6) becomes 500 DEG C, place It is 10 hours to manage the time, the H that use quality score is 1% in step 7)2O2, other conditions are constant to can be prepared by this example catalyst.
Embodiment 6
Phosphorus acid content in step 9) in embodiment 1 is replaced with into 1.0g, the constant this example that can be prepared by of other conditions is urged Agent.
Comparative example 1
Step 6) end will be proceeded in embodiment 1 and can be prepared by the catalyst agent A containing M1 phases and M2 phases simultaneously.
Comparative example 2
Step 8) end will be proceeded in embodiment 1 and can be prepared by pure M1 phase catalysts B.
The catalytic activity of the above-mentioned all catalyst of implementation is shown in Table 1.
Catalyst carries out activity rating using micro passage reaction.Reaction pressure is generally normal pressure, and temperature is 440 DEG C, former Expect that gas group becomes V (C3H8)/V(NH3)/V(O2)/V (He)=6/7/17/70, air speed 6000mLmin-1.Evaluation takes every time 0.2g catalyst is warming up to required temperature, then switches to reaction gas under inert gas atmosphere, in certain temperature and phase It answers and is reacted under air speed, reaction end gas is by the automatic ten-way valve automatic sampling in clack box (240 DEG C), warm pipeline (240 DEG C) on-line analysis on the GC -2060 type gas chromatographs for being equipped with TCD and FID dual detectors, double chromatographic columns.TCD detectors are matched Standby 13 X molecular sieve column and 5A molecular sieve columns, column length are respectively 2m, and high-purity helium makees carrier gas, 80 DEG C of separation detections CO and CO2.FID is examined It surveys device and is equipped with PLOT-Q columns, column length 2m, High Purity Nitrogen makees carrier gas, separation detection propane, propylene, acetonitrile and acrylonitrile at 200 DEG C.Respectively The propane ammoxidation activity evaluation result of kind catalyst is referring to table 1.
1 various catalyst of table are used for the catalytic activity of propane ammoxidation
Embodiment Acrylonitrile yield (%) Acrylonitrile selectivity (%) Conversion ratio
1 53.5 65.6 81.6
2 35.1 55.8 62.9
3 26.7 60.0 44.5
4 31.6 50.4 62.7
5 20.5 70.1 29.2
6 30 73 41.1
Comparative example 1 37.3 59.4 62.8
Comparative example 2 42 52.2 80.5
Reaction condition：Catalyst loading：0.2g, 440 DEG C, normal pressure, V (C3H8)/V(NH3)/V(O2)/V (He)=6/7/ 17/70, air speed GHSV (outlet)=6000mLSTP/(h·g-cat).
As can be seen from Table 1, the MoVTeNb catalyst of P Modification has good catalytic activity, mixed relative to M1+M2 Close phase catalyst comparative example 1 and pure M1 phase catalysts comparative example 2, in the case of high conversion of propane, still maintain compared with High acrylonitrile selectivity, acrylonitrile yield have reached 53.5%.

Claims (9)

1. a kind of Catalyst For Propane Ammoxidation of P Modification, it is characterised in that its chemical general formula is Pa-MobVcTedNbeOx, wherein 0.0001≤a≤1,0.1≤b≤1,0.1≤c≤1,0.1≤d≤1,0.1≤e≤1.
2. a kind of preparation method of the Catalyst For Propane Ammoxidation of P Modification as described in claim 1, it is characterised in that specific Steps are as follows：
1) Mo salt and Te salt are dissolved in the water and solution A is made；
2) V salt is dissolved in the water and solution B is made；
3) Nb salt is dissolved in the water and solution C is made；
4) solution B is added in solution A to and is stirred to obtain mixed solution, described urge can be prepared by adding solution C stirring The slurry of agent；
5) slurry of catalyst obtained in step 4) is subjected to hydro-thermal reaction；Reaction product is obtained through being filtered, washed and drying Catalyst precursor；
6) catalyst precursor obtained in step 5) is subjected to calcination process；
7) by the catalyst precursor H after roasting in step 6)2O2It is handled；
8) by H in step 7)2O2Treated, and catalyst precursor can be prepared by the P Modification by infusion process and phosphorus doping Catalyst For Propane Ammoxidation.
3. the preparation method of the Catalyst For Propane Ammoxidation of P Modification as claimed in claim 2, it is characterised in that：In step 1) The Mo salt is ammonium molybdate；The one kind of the Te salt in telluric chloride and telluric acid.
4. the preparation method of the Catalyst For Propane Ammoxidation of P Modification as claimed in claim 2, it is characterised in that：In step 2) The V salt is selected from one kind of vanadic sulfate and ammonium metavanadate.
5. the preparation method of the Catalyst For Propane Ammoxidation of P Modification as claimed in claim 2, it is characterised in that：In step 3) The one kind of the Nb salt in ammonium niobium oxalate, niobium oxalate and columbium pentachloride.
6. the preparation method of the Catalyst For Propane Ammoxidation of P Modification as claimed in claim 2, it is characterised in that：In step 5) The hydrothermal reaction condition is：Reaction kettle is passed through nitrogen and purges 5~20 minutes in advance, and hydrothermal temperature is 175 DEG C, reaction Time is 1~48 hour.
7. the preparation method of the Catalyst For Propane Ammoxidation of P Modification as claimed in claim 2, it is characterised in that：In step 6) The calcination process condition is：It carries out under an inert atmosphere, calcination temperature is 500~600 DEG C, and roasting time is 1~10h.
8. the preparation method of the Catalyst For Propane Ammoxidation of P Modification as claimed in claim 2, it is characterised in that：In step 7) The H2O2Mass fraction be 1~10%.
9. a kind of Catalyst For Propane Ammoxidation of P Modification as described in claim 1 is in preparing acrylonitrile form propane ammoxidation Using.
CN201810386207.5A 2018-04-26 2018-04-26 Phosphorus-modified propane ammoxidation catalyst, and preparation method and application thereof Expired - Fee Related CN108435223B (en)

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Cited By (1)

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Publication number Priority date Publication date Assignee Title
CN112958125A (en) * 2021-02-08 2021-06-15 淮阴师范学院 Preparation method, product and application of paraffin ammoxidation catalyst based on MXene

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CN1231281A (en) * 1998-03-26 1999-10-13 标准石油公司 Molydenum promoted vanadium-antimony-oxide based catalyst for selective paraffin ammoxidation
JP2007216081A (en) * 2006-02-14 2007-08-30 Asahi Kasei Chemicals Corp Manufacturing method for oxide catalyst
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112958125A (en) * 2021-02-08 2021-06-15 淮阴师范学院 Preparation method, product and application of paraffin ammoxidation catalyst based on MXene

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